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Triethylamine → N-(6-Methoxy-4-methyl-8-quinolinyl)-4-methyl-1-piperazinehexanamide

HRID 542831
ノート
印刷プレビュー

反応式

HRID 542831 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][C:7]([NH:9][C:10]1[CH:11]=[C:12]([O:21][CH3:22])[CH:13]=[C:14]2[C:19]=1[N:18]=[CH:17][CH:16]=[C:15]2[CH3:20])=[O:8].[CH3:23][N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1.C(N(CC)CC)C>C1C=CC=CC=1>[CH3:22][O:21][C:12]1[CH:13]=[C:14]2[C:19](=[C:10]([NH:9][C:7](=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:27]3[CH2:28][CH2:29][N:24]([CH3:23])[CH2:25][CH2:26]3)[CH:11]=1)[N:18]=[CH:17][CH:16]=[C:15]2[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 531671-MethylpiperazineHCID 6120236-Bromo-N-(6-methoxy-4-methyl-8-quinolinyl)hexanamide

生成物 1

HCID 13077513N-(6-Methoxy-4-methyl-8-quinolinyl)-4-methyl-1-piperazinehexanamide収率 53.7%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A mixture of 5.5 g (0.015 mole) of 6-bromo-N-(6-methoxy-4-methyl-8-quinolinyl)hexanamide and 1.8 g (0.018 mole) of N-methylpiperazine in 70 ml of benzene was heated under reflux for 20 hr, treated with 2 ml of triethylamine, and heated for an additional 24 hr. The mixture was allowed to cool, filtered and the filtrate was washed with water, dried and concentrated to dryness in vacuo. The residue was recrystallized twice from n-hexane containing a little toluene and then dried in vacuo at 68° to afford 3.1 g (53%) of the title compound, mp 104°-107°.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hr
  3. temperatureheated for an additional 24 hr
  4. temperatureto cool
  5. filtrationfiltered
  6. washthe filtrate was washed with water
  7. customdried
  8. concentrationconcentrated to dryness in vacuo
  9. customThe residue was recrystallized twice from n-hexane containing a little toluene
  10. customdried in vacuo at 68°

出典と根拠

ORDレコード
ord-15a34611a2e3437ba1064a2cab86f505
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04659708

反応ノート

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